CN113307518B - Setting time and expansion rate cooperative control method for light-burned MgO-doped cement-based material - Google Patents

Setting time and expansion rate cooperative control method for light-burned MgO-doped cement-based material Download PDF

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CN113307518B
CN113307518B CN202110654361.8A CN202110654361A CN113307518B CN 113307518 B CN113307518 B CN 113307518B CN 202110654361 A CN202110654361 A CN 202110654361A CN 113307518 B CN113307518 B CN 113307518B
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citric acid
magnesium citrate
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setting time
expansion rate
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蒋林华
陈磊
邓轶凡
靳卫准
贲询钦
夏锴伦
高颂
职芳芳
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Hohai University HHU
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    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B7/00—Hydraulic cements
    • C04B7/36—Manufacture of hydraulic cements in general
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B7/00—Hydraulic cements
    • C04B7/36—Manufacture of hydraulic cements in general
    • C04B7/48—Clinker treatment

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Abstract

The invention relates to a method for synergistically regulating and controlling the setting time and the expansion rate of a light-burned MgO-doped cement-based material, which belongs to the technical field of cement-based material additives. And (3) fitting by adopting a mathematical model to obtain the relation between the citric acid doping amount X or the magnesium citrate doping amount Y and the coagulation time a and the expansion rate b. Through the model, the setting time a and the expansion rate b of the cement-based material can be regulated, controlled and predicted by changing the citric acid doping amount X and the magnesium citrate doping amount Y of the light-burned MgO cement-based material. In addition, the required citric acid doping amount X and magnesium citrate doping amount Y can be calculated according to the setting time a and the expansion rate b required by engineering, so that the problem of expansion efficiency change caused by the retarder is solved.

Description

Setting time and expansion rate cooperative control method for light-burned MgO-doped cement-based material
Technical Field
The invention belongs to the technical field of cement-based material additives, and particularly relates to a method for synergistically regulating and controlling the setting time and the expansion rate of a light-burned MgO-doped cement-based material.
Background
The light-burned MgO is obtained by calcining magnesite at 700-1000 ℃, and can react with water at normal temperature to generate obvious volume expansion. The phase-specific gravity burned magnesium oxide has higher activity of light burned MgO, large early expansion, small later expansion and smaller problem on volume stability. As an efficient expanding agent, the light-burned MgO is suitable for compensating the temperature reduction shrinkage of large-volume concrete and can effectively prevent the generation of cracks.
The large volume of concrete acts as a poor conductor of heat, and a large amount of hydration heat is accumulated in the interior after the cement in the interior is hydrated, so that the temperature in the interior is increased. As the temperature decreases. Particularly in summer, the temperature of the system can rise rapidly due to the fact that the cement is hydrated too fast due to too high temperature. Therefore, in high-temperature weather construction, the retarder is doped to delay the hydration of cement. The retarder can effectively delay the setting time of cement and inhibit the hydration of the cement, so that the working time at high temperature is prolonged, and the hydration heat release is slowed. Compared with the method of paving the cooling water pipe, the method has simple construction process, and can be used together with the methods of paving the cooling water pipe, using low-temperature cement and the like.
However, the addition of a retarder can diminish the expansion efficiency of the lightly burned MgO. For example, the dam of the old river bottom hydropower station in Guizhou adopts light-burned MgO and ADD-3 air-entraining retarder, but the self-generated volume deformation of the on-site concrete is only about 70 percent of the laboratory data. The reduction of the expansion efficiency causes the internal stress of the structure to be incapable of achieving the expected effect, and the cracks are easier to appear.
Disclosure of Invention
The purpose of the invention is as follows: the invention provides a method for synergistically regulating and controlling the setting time and the expansion rate of a light-burned MgO-doped cement-based material, which can simultaneously regulate and control the setting time of the cement-based material and the expansion efficiency of light-burned MgO in the cement-based material.
The technical scheme is as follows: in order to realize the aim, the method for synergistically regulating and controlling the setting time and the expansion rate of the light-burned MgO-doped cement-based material comprises the following steps of:
1) measuring the coagulation time and expansion rate data under different mixing amounts of citric acid and magnesium citrate through tests;
2) fitting the data obtained in the step 1) through a mathematical model to obtain the relation between the citric acid doping amount X and the magnesium citrate doping amount Y and the coagulation time a and the expansion rate b, and obtaining a fitted curve;
3) calculating the setting time a and the expansion rate b under different citric acid doping amounts X and magnesium citrate doping amounts Y through the fitted curve or calculating the citric acid doping amount X and the magnesium citrate doping amount Y according to the required setting time a and the required expansion rate b;
4) and weighing the required addition amounts of citric acid and magnesium citrate according to the calculated total mass of the cement magnesium oxide multiplied by the addition amounts X and Y, preparing the solution with water, and adding the solution into the cement-based material according to the water-cement ratio required by design.
Further, in the step 4), the formula of the cement magnesium oxide is 10000 parts of the cement magnesium oxide, wherein 9200-10000 parts of cement and 0-800 parts of light-burned MgO are added, and the required addition amounts of citric acid and magnesium citrate are as follows: 0-9 parts of citric acid and 0-9 parts of magnesium citrate, wherein X belongs to the group (0, 0.09 wt%) and Y belongs to the group (0, 0.09 wt%).
Furthermore, the calcination temperature of the light-burned MgO is 700-1000 ℃.
Further, in the step 2), fitting data through a mathematical model specifically comprises the following steps:
the relationship between the setting time a and the expansion rate b and the citric acid concentration X and the magnesium citrate concentration Y is represented by the following formula:
f(X+YE)＝a
F(X，t)+G(YE，t)＝2b
Figure BDA0003110785300000021
wherein: x is the mixing amount of citric acid, Y is the mixing amount of magnesium citrate, and Y isEEquivalent citric acid content, a is coagulation time, b is swelling rate, t is age, MCARelative molecular mass of citric acid, MCMRelative molecular mass of magnesium citrate, f (X + Y)E) For the setting time a with respect to the citrate concentration X + YEF (X, t) is the swelling rate of X citric acid at the dosage of X for t days, G (Y)EAnd t) is the swelling rate of the magnesium citrate Y for t days.
Further, in the step 4), the coagulation time is as follows:
Figure BDA0003110785300000022
Figure BDA0003110785300000023
expansion ratio:
Figure BDA0003110785300000024
wherein X is ∈ [ X ∈ [ ]2，X1]，YE∈[Y1，Y2]。
Equivalent citrate mixing amount of magnesium citrate:
Figure BDA0003110785300000025
wherein X is the mixing amount of citric acid, Y is the mixing amount of magnesium citrate, and Y is the mixing amount of magnesium citrateEIs equivalent citric acid content, a is coagulation time, b is swelling rate, MCARelative molecular mass of citric acid, MCMRelative molecular mass of magnesium citrate; x1，X2The citric acid doping amount used for the test close to the citric acid doping amount X, namely X is the same as X1，X2]；a1，a2Is the mixing amount X of citric acid1And X2The coagulation time of a ∈ [ a ]1，a2]；b1，b2To obtain the citric acid doping amount X through experiments1And X2The swelling rate of the polymer at the next t days, i.e. b ∈ [)2，b1](ii) a Wherein Y is1，Y2The magnesium citrate doping amount used for the test close to the magnesium citrate doping amount Y, namely Y is the same as the [ Y ∈ [)1，Y2]；B1，B2The magnesium citrate mixing amount Y is obtained through tests1And Y2Swelling ratio of t days on lower adjacent line segment, i.e. B belongs to [ B ]1，B2]。
The steps of the regulation and control technology are as follows: the setting time of the cement is measured by respectively adding a certain amount of citric acid or magnesium citrate into the cement, and after data is recorded, function fitting is carried out through mathematical software to obtain a formula for regulating and controlling the setting time of the cement by using the citric acid. Then adding the citric acid or the magnesium citrate with the proportion into the cement-based material doped with a certain amount of light-burned MgO to obtain a curve of the expansion rate changing along with time. According to the setting time curve and the expansion rate change curve, citric acid and magnesium citrate are compounded and mixed into the cement-based material, so that the effects of simultaneously regulating and controlling the setting time and the expansion rate of the light-burned MgO cement-based material are obtained.
The mechanism for synergistically regulating and controlling the setting time and the expansion rate of the light-burned MgO cement-based material by using the citric acid and the magnesium citrate is as follows: citric acid acts as a retarder, the retarding effect of which is mainly due to the effect of citrate. The citrate is adsorbed on the surface of the cement, and the contact area of the moisture and cement particles is reduced due to the steric hindrance effect, so that the setting time is prolonged. In cement-based materials, the hydration of magnesium oxide to form magnesium hydroxide is affected by hydroxide ions and magnesium ions in solution. Citric acid, as an acid, lowers the PH of the system after dissolution, reducing the hydroxide concentration and inhibiting the hydration of magnesium oxide. In contrast to citric acid, magnesium citrate, when added to a cementitious material, does not lower the PH of the system. On the other hand, the magnesium citrate can improve the concentration of magnesium ions in the solution, and the same-ion effect can reduce the solubility of magnesium hydroxide and accelerate the precipitation of the magnesium hydroxide.
The above mechanism shows that the effect of regulating and controlling the coagulation time can be achieved by changing the mixing amount of the citrate. Under the condition of the same citrate doping amount, the effect of regulating and controlling the expansion rate can be achieved by changing the PH value of the system and the content of magnesium ions. This can be briefly summarized as two fundamental principles of regulation: (1) the setting time of the cement material mainly depends on the concentration of citrate, and has little relation with the concentration of cations; (2) citric acid can inhibit the swelling efficiency of magnesium oxide, and magnesium citrate can promote the swelling efficiency of magnesium oxide.
Therefore, adjusting the mixing amount of citric acid and magnesium citrate is the key for controlling the coagulation time and the expansion rate simultaneously.
Has the advantages that: (1) the citric acid and the magnesium citrate are adopted as the retarder, and can play a role in synergistically regulating the setting time and the expansion rate; (2) the retarder can be popularized to other retarders with similar functions and derivatives thereof (3) the idea provided by the invention can be made into related engineering software, machine learning is carried out by inputting a large amount of test data so as to input initial parameters, and the corresponding expansion rate and the corresponding condensation time are predicted, so that the engineering is more intelligent.
Drawings
FIG. 1 is a graph showing the effect of citric acid and magnesium citrate on the 20 ℃ initial setting time of a lightly calcined MgO cement paste containing 5 wt% of citric acid and magnesium citrate;
FIG. 2 is a graph showing the effect of citric acid and magnesium citrate on the final set time at 20 ℃ of a lightly calcined MgO cement paste containing 5 wt% of citric acid and magnesium citrate;
FIG. 3 is a graph showing the effect of citric acid and magnesium citrate on the 20 ℃ expansion of a 5 wt% lightly calcined MgO cement paste.
Detailed Description
The invention is further described with reference to the accompanying drawings and the detailed description.
A method for synergistically regulating and controlling the setting time and the expansion rate of a light-burned MgO-doped cement-based material comprises the following steps: 9200 and 10000 portions of cement, 0 to 800 portions of light burned MgO, 0 to 9 portions of citric acid and 0 to 9 portions of magnesium citrate.
The weight sum of the cement and the light-burned MgO is 10000, and the mixing amount of the citric acid X belongs to (0, 0.09 wt%), the mixing amount of the magnesium citrate Y belongs to (0, 0.09 wt%).
And lightly burning the MgO, wherein the calcining temperature is 700-1000 ℃.
A method for synergistically regulating and controlling the setting time and the expansion rate of a light-burned MgO-doped cement-based material comprises the following steps:
(1) measuring the coagulation time and expansion rate data under different mixing amounts of citric acid and magnesium citrate through tests;
(2) fitting data through a mathematical model to obtain the relationship between the citric acid doping amount X and the magnesium citrate doping amount Y and the coagulation time a and the expansion rate b;
(3) the condensation time a and the expansion rate b under different citric acid doping amounts X and magnesium citrate doping amounts Y can be calculated through the fitted curve; the citric acid content X and the magnesium citrate content Y can also be calculated according to the required setting time a and the required expansion rate b.
The relationship between the setting time a and the expansion rate b and the citric acid concentration X and the magnesium citrate concentration Y is represented by the following formula:
f(X+YE)＝a
F(X，t)+G(YE，t)＝2b
Figure BDA0003110785300000041
wherein: x is the mixing amount of citric acid, Y is the mixing amount of magnesium citrate, and Y isEEquivalent citric acid content, a is coagulation time, b is swelling rate, t is age, MCARelative molecular mass of citric acid, MCMRelative molecular mass of magnesium citrate, f (X + Y)E) For the setting time a with respect to the citrate concentration X + YEF (X, t) is the swelling rate of X citric acid at the dosage of X for t days, G (Y)EAnd t) is the swelling rate of the magnesium citrate Y for t days.
Further refinement, by linear fitting can be obtained:
setting time:
Figure BDA0003110785300000051
expansion ratio:
Figure BDA0003110785300000052
wherein X is ∈ [ X ∈ [ ]2，X1]，YE∈[Y1，Y2]。
Equivalent citrate mixing amount of magnesium citrate:
Figure BDA0003110785300000053
wherein X is the mixing amount of citric acid, Y is the mixing amount of magnesium citrate, and Y is the mixing amount of magnesium citrateEIs equivalent citric acid content, a is coagulation time, b is swelling rate, MCARelative molecular mass of citric acid, MCMRelative molecular mass of magnesium citrate; x1，X2The citric acid doping amount used for the test close to the citric acid doping amount X, namely X is the same as X1，X2]；a1，a2Is the mixing amount X of citric acid1And X2The coagulation time of a ∈ [ a ]1，a2]；b1，b2To obtain the citric acid doping amount X through experiments1And X2The swelling rate of the polymer at the next t days, i.e. b ∈ [)2，b1](ii) a Wherein Y is1，Y2The magnesium citrate doping amount used for the test close to the magnesium citrate doping amount Y, namely Y is the same as the [ Y ∈ [)1，Y2]；B1，B2The magnesium citrate mixing amount Y is obtained through tests1And Y2Swelling ratio of t days on lower adjacent line segment, i.e. B belongs to [ B ]1，B2]。
The citric acid doping amount X and the magnesium citrate doping amount Y are calculated according to the required setting time a and the required expansion rate b, the purpose of cooperatively regulating and controlling the setting time a and the expansion rate b of the lightly burned MgO cement-based material is achieved, and the setting time a and the expansion rate b of the lightly burned MgO cement-based material can also be predicted according to the citric acid doping amount X and the magnesium citrate doping amount Y.
The magnesium oxide in the invention adopts light-burned MgO, and the calcination temperature is 700-1000 ℃.
The citric acid and the magnesium citrate adopted in the invention are anhydrous citric acid and anhydrous magnesium citrate, and if a retarder containing crystal water is adopted, the content of the citrate needs to be converted separately.
Examples
The ambient temperature in the examples was 20 ℃. The magnesium oxide content in the examples is 5% of the total mass fraction of cement and magnesium oxide.
The setting time was measured by incorporating 0, 0.03 wt%, 0.06 wt%, 0.09wt% of citric acid into cement. The effect of citric acid and magnesium citrate of figures 1 and 2 on the initial and final set times at 20 c of 5 wt% MgO-doped cement was tested by incorporating magnesium citrate at 0, 0.03522 wt%, 0.07044 wt%, 0.10544 wt% loading (equivalent 0, 0.03 wt%, 0.06 wt%, 0.09wt% loading of citric acid) into the cement. As shown in fig. 1 and 2, it can be seen that the influence of magnesium ions on the initial and final setting time is not more than 5%, and the retardation effect is mainly controlled by the citrate concentration. For the sake of simplifying the calculation, it can be considered that the delayed coagulation effect of citric acid and magnesium citrate is the same after conversion. The linear function is piecewise fitted with the relation between the coagulation time and the doping amount, and the regulation and control formula of the initial coagulation time and the final coagulation time can be obtained and is shown in table 1. It can be seen that the influence of magnesium ions on the initial and final setting time is not more than 5%, and the retarding effect is mainly controlled by the concentration of citrate.
Table 1 shows the setting time control formula of citric acid and magnesium citrate on cement
Figure BDA0003110785300000061
The swelling ratio was measured by blending citric acid in an amount of 0, 0.03%, 0.06%, 0.09% by weight into 5% magnesia cement. The effect of citric acid and magnesium citrate on the expansion rate at 20 ℃ of a 5 wt% lightly calcined MgO cement paste was measured in fig. 3 by incorporating magnesium citrate at 0, 0.03522 wt%, 0.07044 wt%, 0.10544 wt% loading (equivalent to 0, 0.03 wt%, 0.06 wt%, 0.09wt% loading of citric acid) into a 5% magnesia-doped cement, and as shown in fig. 3, it can be seen that magnesium citrate promotes the expansion of magnesium oxide in the cement and citric acid inhibits the expansion of magnesium oxide in the cement.
Assuming that the initial setting time of the cement needs to be prolonged to 338 minutes and the expansion efficiency needs to be the same as that of the cement without retarder, the amount of the citric acid and the magnesium citrate can be determined to be [0, 0.00003 ] by calculating that X +0.85Y is 0.0003]B is2＝0.000753853，b1＝B1＝0.000849086，B2＝0.000869745，X1＝Y1＝0，X2＝0.0003，Y2Substituting the expansion ratio into 0.0003
Figure BDA0003110785300000062
To obtain
0.000849086＝0.5[(X-0.0003)×0.0000952336040114157/-0.0003+0.000753853+Y×0.0000206585462577076/0.0003+0.000849086]-0.317445347X+0.06886182Y-0.317445347X+0.006886182Y＝-6.04×10-10
The calculation can obtain: 0.0053 wt% of X and 0.0246 wt% of Y; therefore, the mixing amount of the citric acid is 0.0053 wt%, the mixing amount of the magnesium citrate is 0.0246 wt%, the initial setting time is 338 minutes, and the expansion efficiency of the magnesium oxide at 7 days is the same as that of the magnesium oxide without the citric acid. Therefore, according to the regulation and control method, the setting time and the expansion rate of the lightly burned MgO cement-based material can be synergistically regulated and controlled by calculating the mixing amount X of the citric acid and the mixing amount Y of the magnesium citrate.

Claims (4)

1. A method for synergistically regulating and controlling the setting time and the expansion rate of a light-burned MgO-doped cement-based material is characterized by comprising the following steps of:
1) measuring the coagulation time and expansion rate data under different mixing amounts of citric acid and magnesium citrate through tests;
2) fitting the data obtained in the step 1) through a mathematical model to obtain the relation between the citric acid doping amount X and the magnesium citrate doping amount Y and the coagulation time a and the expansion rate b, and obtaining a fitted curve;
3) calculating the setting time a and the expansion rate b under different citric acid doping amounts X and magnesium citrate doping amounts Y through the fitted curve or calculating the citric acid doping amount X and the magnesium citrate doping amount Y according to the required setting time a and the required expansion rate b;
4) weighing the required addition amounts of citric acid and magnesium citrate and water according to the calculated total mass of the cement magnesium oxide multiplied by the doping amounts X and Y to prepare a solution, and adding the solution into the cement-based material according to the water-cement ratio required by design;
in the step 2), the data obtained in the step 1) is fitted through a mathematical model, and the specific steps are as follows: the relationship between the setting time a and the expansion rate b and the citric acid concentration X and the magnesium citrate concentration Y is represented by the following formula:
Figure 225910DEST_PATH_IMAGE001
Figure 415452DEST_PATH_IMAGE002
Figure 876520DEST_PATH_IMAGE003
wherein: x is the mixing amount of citric acid, Y is the mixing amount of magnesium citrate, and Y isEEquivalent citric acid content, a is coagulation time, b is swelling rate, t is age, MCARelative molecular mass of citric acid, MCMIs the relative molecular mass of magnesium citrate, f: (
Figure 260359DEST_PATH_IMAGE004
) As regards the coagulation time a
Figure 705247DEST_PATH_IMAGE004
As a function of (a) or (b),
Figure 167321DEST_PATH_IMAGE005
is the swelling rate of the citric acid mixed amount of X for t days,
Figure 748475DEST_PATH_IMAGE006
is the swelling rate of the magnesium citrate Y after the mixing amount is t days.
2. The method for synergistically regulating and controlling the setting time and the expansion rate of the lightly burned MgO-doped cement-based material according to claim 1, wherein in the step 4), the formula of the cement magnesium oxide is 10000 parts of the cement magnesium oxide, wherein 9200-10000 parts of the cement and 0-800 parts of the lightly burned MgO are respectively, and the mass of the citric acid and the magnesium citrate is as follows: 0-9 parts of citric acid and 0-9 parts of magnesium citrate, wherein X belongs to the group (0, 0.09 wt%) and Y belongs to the group (0, 0.09 wt%).
3. The method for synergistically regulating and controlling the setting time and the expansion rate of the lightly burned MgO-doped cement-based material according to claim 2, wherein the calcination temperature of the lightly burned MgO is 700-1000 ℃.
4. The method for synergistically regulating the setting time and the expansion rate of a lightly burned MgO-doped cement-based material according to claim 1, wherein in the step 2),
setting time:
Figure 286904DEST_PATH_IMAGE007
, X+YE∈[X1，X2]；
expansion ratio:
Figure 907503DEST_PATH_IMAGE008
wherein X ∈ [ X ∈ ]1，X2]，YE∈[Y1，Y2]；
Equivalent citrate mixing amount of magnesium citrate:
Figure 642110DEST_PATH_IMAGE009
；
wherein X is the mixing amount of citric acid, Y is the mixing amount of magnesium citrate, and Y is the mixing amount of magnesium citrateEIs equivalent citric acid content, a is coagulation time, b is swelling rate, MCARelative molecular mass of citric acid, MCMRelative molecular mass of magnesium citrate; x1，X2The citric acid doping amount used for the test close to the citric acid doping amount X, namely X is the same as X1，X2]；a1，a2Is a citric acid blendQuantity X1And X2The coagulation time of a ∈ [ a ]1，a2]；b1，b2To obtain the citric acid doping amount X through experiments1And X2The swelling rate of the polymer at the next t days, i.e. b ∈ [)2，b1](ii) a Wherein Y is1，Y2The magnesium citrate doping amount used for the test close to the magnesium citrate doping amount Y, namely Y is the same as the [ Y ∈ [)1，Y2]；B1，B2The magnesium citrate mixing amount Y is obtained through tests1And Y2Swelling ratio of t days on lower adjacent line segment, i.e. B belongs to [ B ]1，B2]。
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